With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.203714-71-0,Dichloro(2-isopropoxyphenylmethylene)(tricyclohexylphosphine)ruthenium (II),as a common compound, the synthetic route is as follows.,203714-71-0
A dry, 1000-mL, one-necked, round-bottomed flask is equipped with a magnetic stirring bar, rubber septum and an argon inlet. The flask is charged under an argon atmosphere with a solid SIMES x HBF4 2 (35.28 mmol, 13.9 g) and dry n-hexane (400 ml_). A solution of potassium tert-amylate (21.6 ml_, 36.75 mmol) is added from a syringe and the resulting mixture is stirred under argon at room temperature for 1 h. To the resulted solution a solid Hoveyda-Grubbs 1st generation catalyst 1 (29.4 mmol, 17.6 g) is added in one portion. The flask is equipped with a reflux condenser with an argon inlet at the top and the reaction mixture is refluxed for 2 h. The contents of the flask are cooled to room temperature and solid CuCI (51.45 mmol, 5.1 g) is added slowly in three portions and the resulting mixture is refluxed for 2 h. From this point forth, all manipulations are carried out in air.; 1.11. Isolation of the product by crystallization; The reaction mixture is evaporated to dryness and re-dissolved in ethyl acetate (200 ml_). The solution is filtrated through a Buchner funnel with glass frit filled with Celite and then concentrated in vacuo. The residue is dissolved in ambient temp. 1 :10 v/v mixture of CH2CI2 and methanol (220 ml_). After concentration to ca. % of the initial volume using a rotary evaporator (room temperature) crystals are precipitated. These crystals are filtered- off on a Buchner funnel with glass frit. The crystals are washed twice with small portions of CH3OH (-20 ml_), and dried in vacuo to give pure Hoveyda 2nd catalysts 3 (25.3 mmol, 15.81 g). The filtrate after crystallization is evaporated to dryness and crystallized for the second time from CH2CI2 and methanol using the same protocol giving an additional crop of pure Hoveyda 2nd generation catalyst (1.7 mmol, 1.08 g). The total yield of pure Hoveyda-Grubbs 2nd generation catalyst 3 is 92% (27.0 mmol, 16.9 g).
203714-71-0 Dichloro(2-isopropoxyphenylmethylene)(tricyclohexylphosphine)ruthenium (II) 10941020, aruthenium-catalysts compound, is more and more widely used in various.
Reference£º
Patent; BOEHRINGER INGELHEIM INTERNATIONAL GMBH; BOEHRINGER INGELHEIM PHARMA GMBH & CO. KG; WO2007/54483; (2007); A1;,
Highly efficient and robust molecular ruthenium catalysts for water oxidation
Catalysts | Special Issue : Ruthenium Catalysts – MDPI